US3890426A - Method of treating alunite ore - Google Patents

Method of treating alunite ore Download PDF

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Publication number
US3890426A
US3890426A US453225A US45322574A US3890426A US 3890426 A US3890426 A US 3890426A US 453225 A US453225 A US 453225A US 45322574 A US45322574 A US 45322574A US 3890426 A US3890426 A US 3890426A
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United States
Prior art keywords
liquid
precipitation
aluminum hydroxide
sulfate
aluminum
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Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US453225A
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English (en)
Inventor
Douglas Stevens
Helge O Forberg
Larry D Jennings
Jr Frank M Stephens
Francis J Bowen
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Southwire Co LLC
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Southwire Co LLC
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Publication date
Application filed by Southwire Co LLC filed Critical Southwire Co LLC
Priority to US453225A priority Critical patent/US3890426A/en
Priority to NO750859A priority patent/NO750859L/no
Priority to AU79118/75A priority patent/AU484811B2/en
Priority to CA222,357A priority patent/CA1066025A/en
Priority to BR1673/75A priority patent/BR7501673A/pt
Priority to FR7508715A priority patent/FR2274559A1/fr
Priority to JP3418975A priority patent/JPS5623925B2/ja
Priority to ES435868A priority patent/ES435868A1/es
Priority to GB11979/75A priority patent/GB1488292A/en
Priority to AR258083A priority patent/AR202444A1/es
Priority to IT48715/75A priority patent/IT1047763B/it
Application granted granted Critical
Publication of US3890426A publication Critical patent/US3890426A/en
Anticipated expiration legal-status Critical
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F7/00—Compounds of aluminium
    • C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
    • C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
    • C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
    • C01F7/0686—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process from sulfate-containing minerals, e.g. alunite

Definitions

  • the present invention concerns a method of recovering aluminum hydroxide from ore containing alunite by calcination, leaching with a weak base, digestion with a mixture of sodium hydroxide and potassium hydroxide and a subsequent precipitation of aluminum hydroxide by cooling and seeding the resultant solution.
  • U.S. Pat. No. 1,948,887 (Saunders) is representative of prior art techniques.
  • U.S. Pat. No. 1,406,890 (Pederson) further discloses the precipitation of potash alum" by the addition of potassium sulfate to an acidic leach solution.
  • Loevenstein in U.S. Pat. No. 2,958,580 teaches the recovery of aluminum as aluminum sulfate by digesting aluminum ore with sulfuric acid.
  • the present invention concerns a method for recovering aluminum hydroxide from ore containing alunite by using a low temperature roast followed by leaching with a weak base and digestion with a mixture of sodium hydroxide and potassium hydroxide.
  • One object of the present invention is to provide a novel method for economically extracting aluminum hydroxide from ore containing alunite.
  • a further object of this invention is to provide a novel and economical method for separating aluminum hydroxide from ore containing alunite which consists of aluminum, potassium, sodium, sulfates and water.
  • FIG. 1 is a general diagrammatic representation of an embodiment of the present invention.
  • FIG. 2 is a diagrammatic representation of an embodiment of the present invention depicting bi-product recovery.
  • FIG. 3 is a diagramatic representation of an embodiment of the present invention depicting an optional method of silica removal.
  • FIG. 1 is a general diagramatic flow sheet of an embodiment of this invention, ore containing what is commonly known as alunite, which has an approximate empirical formula of [K AI (OH Na Al (OH), (SO and/or combinations thereof, is roasted to remove the water of hydration, leached with a weak base, and the liquid and solid components separated.
  • the solid product of this separation is then digested with a mixture of alkali metal hydroxides and the liquid and solid components separated in a second separation step.
  • the liquid portion resulting from the second separation is then seeded or heated to remove silica by precipitating sodium aluminum silicate.
  • the remaining liquid is then cooled and/or seeded to precipitate and recover aluminum hydroxide.
  • the alunite ore is roasted in the roasting step at a temperature of from about 400C to about 850C, preferably the ore is roasted at a temperature of from about 500C to about 650C, in order to effect removal of the water of hydration.
  • the roasting step is carried out at atmospheric pressure and the preferred temperature is maintained for from about one half minute to about six hours. The residence time within the roasting step varies greatly depending upon the type equipment used.
  • the roasted ore is advantageously leached with a base selected from the group consisting of ammonium hydroxide and alkali metal hydroxides at a pH of between about 8 and about 12 to dissolve sulfates and alkali metals.
  • a base selected from the group consisting of ammonium hydroxide and alkali metal hydroxides at a pH of between about 8 and about 12 to dissolve sulfates and alkali metals.
  • the leaching step is carried out at a temperature of up to about C and for a time of from about five minutes to about two hours.
  • Ammonium hydroxide is the most preferred base for use in the leaching step, and the preferred concentration is from about 12.5 to about 32 grams free ammonia per liter of solution.
  • the liquid and solid components from the leaching step are separated in the first separation step by conventional means such as thickener tanks, filters, belt extractor filters, and the like.
  • the solid content separated is then digested with a mixture of alkali metal hydroxides having a concentration of up to about 300 grams per liter caustic expressed as Na CO
  • the alkali metal hydroxides are sodium hydroxide and potassium hydroxide.
  • the mixture ratio can vary from about 20 percent to about 100 percent sodium hydroxide, to about 80 percent to about 0 percent potassium hydroxide.
  • the mixture contains in excess of 50 percent sodium hydroxide.
  • the digestion conditions are atmospheric pressure, a temperature of from about 80C to about C, and a digestion time of from about five minutes to about two hours.
  • the digestion product is then separated in the second separation step by conventional methods such as thickener tanks, filters, and the like.
  • Excess silica is then removed from the separated liquid content by heating the liquid and/or by seeding the liquid with sodium aluminum silicates.
  • Advantageously agitation is applied to this liquid portion during the removal of excess silica. If atmospheric pressure is used in the heating step a temperature of about 90C for a time of at least one hour is required. If pressure in excess of atmospheric pressure is used a temperature of from about 90C to about 200C is required to precipitate the sodium aluminum silicate in a time of at least minutes.
  • the heating is carried out at a pressure of from about 0.5 atmosphere to about 7 atmospheres.
  • Aluminum hydroxide seed crystals may then be added to the solution and upon cooling crystals of aluminum hydroxide are formed, precipitated and are separated from the solution as crystalline aluminum hydroxide.
  • the alunite ore Prior to the roasting step the alunite ore optionally may be crushed to a particle size having a greatest distance between parallel opposite exterior surfaces of about one inch or less.
  • the product may be ground to a particle size of about eight mesh or less subsequent to the roasting step.
  • the liquid from the first separation step optionally may be processed by vacuum or cooling crystallization to precipitate a mixture of ammonium sulfate and potassium sulfate when ammonia is the weak base employed in the leaching step, or sodium and potassium sulfate when sodium hydroxide and potassium hydroxide are the base.
  • ammonia the weak base employed in the leaching step
  • sodium and potassium sulfate when sodium hydroxide and potassium hydroxide are the base.
  • ammonia the preferred base
  • the mixture of ammonium sulfate and potassium sulfate is removed from the solution by filtering, centrifuging or the like.
  • the mixed salts can either be marketed as such or fed to the pyrolysis unit shown in FIG.
  • the pyrolysis unit can be a fluidized bed reactor, a rotating kiln, a shaft furnace or the like. Vapors from the pyrolysis unit are then passed through a column of pebble lime which reacts with the sulfur trioxide produced by the pyrolysis to form calcium sulfate. The ammonia and water produced by the pyrolysis are also passed through the lime column before being recycled to the weak base leaching step. Calcium sulfate so produced can then be either prepared for marketing or discarded as a waste.
  • the liquid content separated in the first separation step of FIG. 2 optionally may be processed by adding a weak base, such as ammonia, thereby precipitating potassium sulfate.
  • the liquid may then be boiled in a lime boil step in the presence of lime [Ca(OH) preferably in excess of stoichiometric amounts at atmospheric pressure, a reaction time of from about fifteen minutes to about one and one-half hours.
  • the product of the lime boil step is then separated by conventional means such as centrifuge, filter, thickener tanks, vacuum distillation or crystallization, and the like.
  • the liquid portion then can be recycled to use in the leaching step and the solid precipitated sulfate converted to commercial products such as sulfuric acid, elemental sulfur and the like.
  • the product formed in the silica removal step optionally may be filtered and the liquid solution containing aluminum hydroxide transferred to the precipitation step.
  • the solid content filtered is sodium aluminum silicate with or without a sulfate ion depending upon the concentration of silicon and sulfate in the solution.
  • the resultant liquid is cooled to precipitate crystalline aluminum hydroxide, which is then separated from the liquid.
  • the liquid is seeded with aluminum hydroxide crystals during the cooling step to accelerate the rate of precipitation and control the particle size of crystalline aluminum hydroxide.
  • the liquid from the precipitation step of FIG. 2 (sodium and potassium hydroxide) optionally may be recycled and used in the digestion step.
  • the solid content of the precipitation step may be washed with water or with a dilute acid.
  • the aluminum hydroxide product from the precipitation step of FIG. 1 optionally may be calcined (heated) to form alumina (M 0
  • alumina M 0
  • a quantity of leached alunite calcine was digested as in Example No. 1. Boiling temperatures were used to insure maximum alumina digestion. A paddle stirer was used to provide agitation. After digestion, the mixture was filtered by suction.
  • the proportions were 1200 milliliters of 250 grams per liter NaOH and 600 grams of leached alunite calcine. Due to test losses, only about 850 milliliters of liquor were obtained. Enough demineralized water was added by washing the filter cake to provide one liter of liquor. At this point the solution contained 200 gm/l free caustic, 91 gm/l A1 0 and 3.60 gm/l SiO 143 grams of the ammonia leach residue were digested in 340 ml of mixed caustic having a caustic concentration of 220 grams per liter as Na CO The slurry was boiled at a pressure of one atmosphere with mechanical agitation for 60 minutes and filtered.
  • a method for recovering aluminum hydroxide from ore containing alunite comprising the steps of:
  • Step (c) digesting the solid portion from Step (c) with an aqueous mixture of alkali metal hydroxides at a concentration and at a temperature sufficient to extract the aluminum content from said solid portion.
  • Step (a) is performed at a temperature of from about 400C to about 850C.
  • Step (a) is performed at a temperature of from about 500C to about 650C.
  • Step (b) is selected from the group consisting of ammonium hydroxide and alkali metal hydroxides.
  • Step (b) is performed at a temperature of from about C to about 120C and for a time of at least five minutes.
  • alkali metal hydroxides of Step (d) are selected from the group consisting of sodium hydroxide and potassium hydroxide.
  • Step (h) The method of claim 1 in which the precipitation of aluminum hydroxide in Step (h) is performed by cooling the liquid until crystalline aluminum hydroxide is formed.
  • Step (h) The method of claim 1 further including accelerating the precipitation of aluminum hydroxide in Step (h) by seeding the liquid with aluminum hydroxide crystals.
  • Step (f) The method of claim 1 including the additional step of filtering the solution formed in Step (f) to yield sodium aluminum silicate solids and sodium aluminum sulfate solids.

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  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Geology (AREA)
  • Inorganic Chemistry (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)
US453225A 1974-03-21 1974-03-21 Method of treating alunite ore Expired - Lifetime US3890426A (en)

Priority Applications (11)

Application Number Priority Date Filing Date Title
US453225A US3890426A (en) 1974-03-21 1974-03-21 Method of treating alunite ore
NO750859A NO750859L (enrdf_load_stackoverflow) 1974-03-21 1975-03-13
AU79118/75A AU484811B2 (en) 1974-03-21 1975-03-14 Method of treating alunite ore
CA222,357A CA1066025A (en) 1974-03-21 1975-03-18 Method of treating alunite ore
FR7508715A FR2274559A1 (fr) 1974-03-21 1975-03-20 Recuperation d'hydroxyde d'aluminium par traitement de minerais contenant de l'alunite
JP3418975A JPS5623925B2 (enrdf_load_stackoverflow) 1974-03-21 1975-03-20
BR1673/75A BR7501673A (pt) 1974-03-21 1975-03-20 Processo para a recuperacao de hidroxido de aluminio
ES435868A ES435868A1 (es) 1974-03-21 1975-03-21 Procedimiento para recuperar hidroxido de aluminio de mine-ral que contiene alunita.
GB11979/75A GB1488292A (en) 1974-03-21 1975-03-21 Method of treating alunite ore
AR258083A AR202444A1 (es) 1974-03-21 1975-03-21 Procedimiento para la recuperacion de aluminio de un mineral conteniendo alunita en forma de hidroxido de aluminio
IT48715/75A IT1047763B (it) 1974-03-21 1975-03-21 Metodo per il trattamento di una roccia contenente allunite

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US453225A US3890426A (en) 1974-03-21 1974-03-21 Method of treating alunite ore

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US (1) US3890426A (enrdf_load_stackoverflow)
JP (1) JPS5623925B2 (enrdf_load_stackoverflow)
AR (1) AR202444A1 (enrdf_load_stackoverflow)
BR (1) BR7501673A (enrdf_load_stackoverflow)
CA (1) CA1066025A (enrdf_load_stackoverflow)
ES (1) ES435868A1 (enrdf_load_stackoverflow)
FR (1) FR2274559A1 (enrdf_load_stackoverflow)
GB (1) GB1488292A (enrdf_load_stackoverflow)
IT (1) IT1047763B (enrdf_load_stackoverflow)
NO (1) NO750859L (enrdf_load_stackoverflow)

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3996334A (en) * 1975-06-02 1976-12-07 Southwire Company Process for recovering aluminum from alunite
US3996333A (en) * 1975-08-28 1976-12-07 Southwire Company Method for dehydrating ores
US4008307A (en) * 1975-06-02 1977-02-15 Southwire Company Production of monobasic potassium phosphate by ion exchange
US4029737A (en) * 1976-04-09 1977-06-14 Southwire Company Redox treatment of alunite ore
US4057611A (en) * 1975-12-24 1977-11-08 Southwire Company Process for recovering aluminum from alunite
US4064217A (en) * 1976-09-30 1977-12-20 Hartman George J Process for recovering aluminum from alunite ore
US4075068A (en) * 1976-07-12 1978-02-21 Southwire Company Process for the recovery of aluminum from alunite
US4093700A (en) * 1976-02-04 1978-06-06 Southwire Company Process for reduction of alunite ore in aluminum recovery process
US4173622A (en) * 1978-01-03 1979-11-06 Fmc Corporation Zeolite A crystals of uniformly small particle size and the manufacture thereof
US4230678A (en) * 1979-02-14 1980-10-28 Earth Sciences, Inc. Process for recovering aluminum from alunite
US4618480A (en) * 1984-08-15 1986-10-21 Resource Technology Associates Recovery of alumina values from alunite ore
US5554352A (en) * 1995-05-09 1996-09-10 Construction Material Resources Processed silica as a natural pozzolan for use as a cementitious component in concrete and concrete products
WO2013131317A1 (zh) * 2012-03-07 2013-09-12 深圳市新星轻合金材料股份有限公司 以钾基钛硼氟盐混合物为中间原料生产硼化钛并同步产出钾冰晶石的循环制备方法

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1070324A (en) * 1912-01-13 1913-08-12 Howard F Chappell Manufacture of sulfate of potash and alumina.
US1189254A (en) * 1916-03-21 1916-07-04 Mineral Products Corp Production of aluminates from alunite.
US1191105A (en) * 1916-01-18 1916-07-11 Paul R Hershman Process of producing alluminate from alunite.
US1195655A (en) * 1916-08-22 Poration
US2120840A (en) * 1934-08-20 1938-06-14 Bohn Aluminium & Brass Corp Cyclic process for treating alunite
US2398425A (en) * 1943-04-27 1946-04-16 Elnathan H Steinman Process for treating alunite ores and the like
US3652208A (en) * 1970-05-04 1972-03-28 Trw Inc Alumina extraction from alumino-silicate ores and potassium sulfate ores

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US1195655A (en) * 1916-08-22 Poration
US1070324A (en) * 1912-01-13 1913-08-12 Howard F Chappell Manufacture of sulfate of potash and alumina.
US1191105A (en) * 1916-01-18 1916-07-11 Paul R Hershman Process of producing alluminate from alunite.
US1189254A (en) * 1916-03-21 1916-07-04 Mineral Products Corp Production of aluminates from alunite.
US2120840A (en) * 1934-08-20 1938-06-14 Bohn Aluminium & Brass Corp Cyclic process for treating alunite
US2398425A (en) * 1943-04-27 1946-04-16 Elnathan H Steinman Process for treating alunite ores and the like
US3652208A (en) * 1970-05-04 1972-03-28 Trw Inc Alumina extraction from alumino-silicate ores and potassium sulfate ores

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3996334A (en) * 1975-06-02 1976-12-07 Southwire Company Process for recovering aluminum from alunite
US4008307A (en) * 1975-06-02 1977-02-15 Southwire Company Production of monobasic potassium phosphate by ion exchange
US3996333A (en) * 1975-08-28 1976-12-07 Southwire Company Method for dehydrating ores
US4057611A (en) * 1975-12-24 1977-11-08 Southwire Company Process for recovering aluminum from alunite
US4093700A (en) * 1976-02-04 1978-06-06 Southwire Company Process for reduction of alunite ore in aluminum recovery process
US4029737A (en) * 1976-04-09 1977-06-14 Southwire Company Redox treatment of alunite ore
US4075068A (en) * 1976-07-12 1978-02-21 Southwire Company Process for the recovery of aluminum from alunite
US4064217A (en) * 1976-09-30 1977-12-20 Hartman George J Process for recovering aluminum from alunite ore
US4173622A (en) * 1978-01-03 1979-11-06 Fmc Corporation Zeolite A crystals of uniformly small particle size and the manufacture thereof
US4230678A (en) * 1979-02-14 1980-10-28 Earth Sciences, Inc. Process for recovering aluminum from alunite
US4618480A (en) * 1984-08-15 1986-10-21 Resource Technology Associates Recovery of alumina values from alunite ore
US5554352A (en) * 1995-05-09 1996-09-10 Construction Material Resources Processed silica as a natural pozzolan for use as a cementitious component in concrete and concrete products
WO2013131317A1 (zh) * 2012-03-07 2013-09-12 深圳市新星轻合金材料股份有限公司 以钾基钛硼氟盐混合物为中间原料生产硼化钛并同步产出钾冰晶石的循环制备方法

Also Published As

Publication number Publication date
BR7501673A (pt) 1975-12-16
FR2274559A1 (fr) 1976-01-09
FR2274559B1 (enrdf_load_stackoverflow) 1977-04-15
ES435868A1 (es) 1976-12-16
AU7911875A (en) 1976-09-16
JPS5623925B2 (enrdf_load_stackoverflow) 1981-06-03
CA1066025A (en) 1979-11-13
JPS50131894A (enrdf_load_stackoverflow) 1975-10-18
GB1488292A (en) 1977-10-12
IT1047763B (it) 1980-10-20
NO750859L (enrdf_load_stackoverflow) 1975-09-23
AR202444A1 (es) 1975-06-06

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